DE10309221A1 - Leveling agent for dyeing fibers - Google Patents

Abstract

The present invention relates to a composition comprising at least one amine salt of an alkylarylsulfonate and at least one alkoxylated alkylamine, which can be used as a leveling agent for dyeing fiber materials, and a process for their preparation. In addition, the present invention relates to colorants which contain the leveling agents according to the invention.

Description

The present invention relates to a composition used as a leveling agent for dyeing fiber materials can be used, as well as a process for their preparation. About that In addition, the present invention relates to coloring agents which are the leveling agents according to the invention contain.

Textile materials are common colored, for example, plain or patterned. The setting a color is usually done by a combination of several, for example two or three dyes.

Especially with colored floor coverings However, textile materials have the disadvantage that they are under Shoot the influence of light and the warming caused by the light. Under Shooting understands one a color change of the flooring, which is due that a color component of a dye combination due to the influence of light of color intensity stronger loses than the other dyes. Especially with flooring in buildings huge Glass fronts are often worn out after a few years. This problem lies not only with floor coverings, but with every geometric one Fiber structures before.

To fire prematurely Avoiding textile materials are often particularly lightfast dyes used. Therefore come, for example, metal complex dyes because of their high fastness to hot light or trichromes from very lightfast acid dyes in question. Indeed it is particularly great when using trichromes lightfast acid dyes difficult to evenly dye the dyes with known leveling aids no matter to pull on the respective fiber.

In the DE-A-23 43 418 For example, the coloring of polyamide or polyamide-containing goods with particularly real dyes is described. For this purpose, leveling aids based on salts of sulfonic acid group-containing surfactants in combination with oxyethylated polyamides have been described. However, these leveling aids, which have only a fiber-affine effect, only lead to unsatisfactory results because they have no synchronizing effect and have no influence on the absorption behavior of the dyes.

The object of the present invention is thus providing a composition that is both at least contains a fiber-affine component, which has an equalizing effect on the fiber, as well influences the dipping behavior of the dyes. Through the The effect of the composition is said to be the different winding behavior of individual dyes in color formulations are synchronized as well as the uniformity the coloring be secured.

According to the invention, it was found that a composition containing at least one amine salt of an alkyl aryl sulfonate and contains at least one alkoxylated alkylamine that meets the above requirements.

Object of the present invention is thus a composition comprising at least one amine salt Contains alkylarylsulfonate and at least one alkoxylated alkylamine.

Alkylarylsulfonate amine salt:

The alkylarylsulfonate contained in the composition according to the invention preferably has a linear, branched or partially branched C ₁ -C ₃₆ -alkyl radical and a C ₆ -C ₁₂ -aryl radical. The synthesis of these alkylarylsulfonates can, for example, according to the DE-A-102 48 002 respectively.

in der R¹ für einen linearen, verzweigten oder teilverzweigten C₁-C₃₆-Alkylrest, bevorzugt C₈-C₂₄-Alkylrest, besonders bevorzugt C₁₀-C₂₀-Alkylrest, steht,
R², R³, R⁴ unabhängig voneinander für Wasserstoff, C₁-C₁₆-Alkyl, vorzugsweise C₁-C₁₂-Alkyl, besonders bevorzugt C₁-C₈-Alkyl, C₆-C₁₀-Aryl, besonders bevorzugt Phenylen, Heteroaryl, Hydroxyalkyl, C₂-C₅-Alkanol, besonders bevorzugt C₂- oder C₃-Alkanol, stehen, und
m für 1, 2 oder 3 steht.The alkylarylsulfonate used in the composition according to the invention preferably corresponds to the general formula (I)

in which R ^{1 is} a linear, branched or partially branched C ₁ -C ₃₆ -alkyl radical, preferably C ₈ -C ₂₄ -alkyl radical, particularly preferably C ₁₀ -C ₂₀ -alkyl radical,
R ² , R ³ , R ⁴ independently of one another for hydrogen, C ₁ -C ₁₆ alkyl, preferably C ₁ -C ₁₂ alkyl, particularly preferably C ₁ -C ₈ alkyl, C ₆ -C ₁₀ aryl, particularly preferred Phenylene, heteroaryl, hydroxyalkyl, C ₂ -C ₅ alkanol, particularly preferably C ₂ or C ₃ alkanol, and
m stands for 1, 2 or 3.

If the alkylarylsulfonate has a branched alkyl radical R ¹ , it is preferably a C ₁ -C ₄ -branched alkyl radical, particularly preferably a methyl- or ethyl-branched alkyl radical.

Is it the alkyl residue of the alkylarylsulfonate around a partially branched alkyl radical, the degree of branching is preferably 0.1 to 4, particularly preferably 0.5 to 2, in particular 1 to 1.5.

The alkyl radicals R ¹ are, for example, n-octyl, iso-octyl, tert.-octyl, 2-ethylhexyl, Nonyl or pelargonyl, decyl or caprinyl, undecyl, dodecyl or lauryl, myristyl, palmityl or hexadecyl or stearyl. Dodecyl is particularly preferred.

In a special embodiment The present invention is the ethanolamine salt of dodecylbenzenesulfonate.

The amine salt of alkylarylsulfonate acts in the composition according to the invention essentially affinity for fibers.

Alkoxylated alkylamine:

The alkoxylated alkylamine is preferably obtainable by reacting a C ₁ -C ₃₆ alkylamine, particularly preferably C ₈ -C ₂₄ alkylamine, in particular C ₁₀ -C ₂₀ alkylamine, with an average of 2 to 100 mol, preferably 5 to 50 mol, particularly preferably 10 to 15 mol, of at least one alkylene oxide.

According to the invention are suitable for alkoxylation all primary and secondary Alkyl amines. Examples of this are methylamine, ethylamine, n-propylamine, isopropylamine, n-butylamine, iso-butylamine, tert-butylamine, n-pentylamine, cyclopentylamine, isopentylamine, n-hexylamine, Cyclohexylamine, n-octylamine, n-decylamine, 1-phenylethylamine, 2-phenylethylamine, Allylamine, 2-methoxyethylamine, dimethylamine, diethylamine, di-n-propylamine, Diisopropylamine, di-n-butylamine, pyrolidine, piperidine, hexamethyleneamine, Piperazine, morpholine, monoethylamine, diethylamine, triethylamine, n-propylamine, di-n-propylamine, iso-propylamine, diisopropylamine, n-butylamine, di-n-butylamine, isobutylamine, tert-butylamine, n-pentylamine, isopentylamine and oleylamine.

The alkylamine is preferably in Agents with 2 to 100 mol, particularly preferably 5 to 50 mol, in particular 10 to 15 mol, implemented at least one alkylene oxide. In principle, you can do this all alkylene oxides are used which are known to the person skilled in the art. Examples are substituted or unsubstituted alkylene oxides 2 to 24 carbon atoms, such as alkylene oxides with halogen, hydroxy, not cyclic ether or ammonium substituents. In particular are too name: aliphatic 1,2-alkylene oxides with 2 to 4 carbon atoms, for example Ethylene oxide, propylene oxide, 1,2-butylene oxide, 2,3-butylene oxide or Isobutylene oxide, aliphatic 1,2-alkylene oxides with 5 to 24 carbon atoms, cycloaliphatic alkylene oxides, for example cyclopentene oxide, Cyclohexene oxide or cyclododecatriene (1,5,9) monoxide, araliphatic Alkylene oxides, for example styrene oxide.

Examples of substituted alkylene oxides are epichlorohydrin, epibromohydrin, 2,3-epoxy-1-propanol, 1-allyloxy-2,3-epoxypropane, 2,3-epoxyphenyl ether, 2,3-epoxypropyl isopropyl ether, 2,3-epoxypropyl octyl ether or 2,3-epoxypropyltrimethyl-ammonium chloride.

Are particularly preferred for the method according to the invention 1,2-alkylene oxides used with 2 to 4 carbon atoms, especially ethylene oxide and / or propylene oxide.

in der:
X Ethylenoxideinheiten – (CH₂CH₂O)_n – mit im Mittel vorzugsweise n = 2 bis 100, besonders bevorzugt n = 5 bis 50, insbesondere n = 10 bis 15, bedeutet oder
X Propylenoxideinheiten – (CH₂CH₂CH₂O)_n – mit im Mittel vorzugsweise n = 2 bis 100, besonders bevorzugt n = 5 bis 50, insbesondere n = 10 bis 15, bedeutet oder
X eine gemischte Gruppe aus Ethylenoxid- und Propylenoxideinheiten mit einer Monomerenanzahl von im Mittel vorzugsweise 2 bis 100, besonders bevorzugt 5 bis 50, insbesondere 10 bis 15, bedeutet. Die Ethylen- und Propylenoxideinheiten können dabei im alkoxylierten Alkylamin statistisch oder als Blöcke vorliegen. Unter statistisch wird erfindungsgemäß verstanden, dass die Ethylen- und Propyleneinheiten in beliebiger Reihenfolge in dem alkoxylierten Alkylamin vorliegen. Liegen die Ethylen- und Propyleneinheiten als Blöcke vor, so kann es sich um homogene (nur Ethylen- oder Propylenoxideinheiten) oder heterogene Blöcke (gemischte Blöcke aus Ethylen- und Propylenoxideinheiten) handeln.In a preferred embodiment, the alkoxylated alkylamine thus has the general structural unit (II)

in the:
X is ethylene oxide units - (CH ₂ CH ₂ O) _n - with on average preferably n = 2 to 100, particularly preferably n = 5 to 50, in particular n = 10 to 15, or
X propylene oxide units - (CH ₂ CH ₂ CH ₂ O) _n - with on average preferably n = 2 to 100, particularly preferably n = 5 to 50, in particular n = 10 to 15, or
X is a mixed group of ethylene oxide and propylene oxide units with an average number of monomers of preferably 2 to 100, particularly preferably 5 to 50, in particular 10 to 15. The ethylene and propylene oxide units can be present statistically or as blocks in the alkoxylated alkylamine. According to the invention, statistical means that the ethylene and propylene units are present in the alkoxylated alkylamine in any order. If the ethylene and propylene units are in the form of blocks, they can be homogeneous (only ethylene or propylene oxide units) or heterogeneous blocks (mixed blocks of ethylene and propylene oxide units).

The alkoxylated alkylamine works in the composition according to the invention essentially dye affinity.

Alkoxylated alcohol:

In a special embodiment of the present invention the composition according to the invention additionally at least one alkoxylated alkyl alcohol.

The alkoxylated alkyl alcohol preferably has a C ₁ -C ₃₆ alkyl radical, particularly preferably C ₈ -C ₂₄ alkyl radical, in particular C ₁₀ -C ₂₀ alkyl radical. The alkyl radicals of the alkyl alcohol are, for example, n-octyl, iso-octyl, tert-octyl, 2-ethylhexyl, nonyl or pelargonyl, decyl or caprinyl, undecyl, dodecyl or lauryl, myristyl, palmityl or hexadecyl , Stearyl.

The alkoxylated alkyl alcohol is preferably obtainable by reacting a C ₁ -C ₃₆ -alkyl alcohol with an average of 2 to 100 mol, particularly preferably 5 to 50 mol, in particular 10 to 15 mol, of at least one alkylene oxide. In principle, all alkylene oxides known to the person skilled in the art can be used for this. Examples are substituted or unsubstituted alkylene oxides with 2 to 24 carbon atoms, such as alkylene oxides with halogen, hydroxyl, non-cyclic ether or ammonium substituents. Particular mention should be made of: aliphatic 1,2-alkylene oxides with 2 to 4 carbon atoms, for example ethylene oxide, propylene oxide, 1,2-butylene oxide, 2,3-butylene oxide or isobutylene oxide, aliphatic 1,2-alkylene oxides with 5 to 24 carbon atoms Atoms, cycloaliphatic alkylene oxides, for example cyclopentene oxide, cyclohexene oxide or cyclododecatriene (1,5,9) monoxide, araliphatic alkylene oxides, for example styrene oxide.

Examples of substituted alkylene oxides are epichlorohydrin, epibromohydrin, 2,3-epoxy-1-propanol, 1-allyloxy-2,3-epoxypropane, 2,3-epoxy-phenyl ether, 2,3-epoxypropyl isopropyl ether, 2,3-epoxypropyl octyl ether or 2,3-epoxypropyltrimethyl-ammonium chloride.

1,2-alkylene oxides are particularly preferred with 2 to 4 carbon atoms, especially ethylene oxide and / or propylene oxide.

Alternatively, it is also possible that the alkoxylated alkyl alcohol mixed alkylene oxide units, preferably Ethylene and propylene oxide units. The mixed alkylene oxide units can are present statistically or as blocks in the alkoxylated alkyl alcohol.

The alkoxylated alkyl alcohol works in the composition according to the invention essentially affinity for fibers.

Composition:

In the compositions according to the invention it is preferably aqueous compositions. alternative but it can also be alcoholic compositions or mixtures both act.

In a preferred embodiment of the present invention the content of the amine salt of the alkylarylsulfonate in the composition according to the invention 20 to 70 wt .-%, preferably 30 to 50 wt .-%, particularly preferred 40 to 45 wt .-%, each based on the composition of the invention. The content of alkoxylated alkylamine in the composition according to the invention is preferably 1 to 20% by weight, particularly preferably 2 to 10% by weight, in particular 2.5 to 5% by weight, in each case based on the composition according to the invention. The content of alkoxylated alkyl alcohol in the composition according to the invention is preferably 0 to 20% by weight, particularly preferably 1 to 5% by weight, in particular 2.5 to 5 wt .-%, each based on the composition of the invention. The total weight of the composition is 100% by weight.

The composition according to the invention can optionally contain other additives. Examples of these are acids, polyols and solvent promoters, such as polyalkylene oxides.

Another subject of the present Invention is a process for the preparation of the composition according to the invention. For this purpose, at least one amine salt of an alkylarylsulfonate, at least one alkoxylated alkylamine and optionally at least an alkoxylated alkyl alcohol mixed together. Regarding more specific versions to the amine salt of an alkyl aryl sulfonate, the alkoxylated alkyl amine and the alkoxylated alkyl alcohol is based on the above statements in terms of the composition of the invention directed.

Another object of the invention is the use of the composition according to the invention as a leveling aid.

Under a leveling aid for the purposes of the present invention, a composition is understood which have both a leveling effect and a synchronization effect when dyeing one fiber shows.

Understands a leveling effect the mobility of the dyes in the sense of the present invention on a fiber. A synchronization effect is understood the adjustment of the speed at which the dyes are drawn up.

Another subject of the present Invention are leveling aids which have a composition according to the invention contain.

Another subject of the present Invention is the use of these leveling aids for dyeing Fibers.

Let the leveling agents according to the invention itself as an aid to dyeing of all fibers known to those skilled in the art, natural or synthetic Use origin. The leveling aids according to the invention are preferably suitable for coloring of synthetic fibers. Examples of suitable according to the invention Fibers are cellulose fibers, polyester fibers, polyacrylonitrile fibers, Polyurethane fibers, acetate fibers, wool fibers and polyamide fibers. The leveling aids according to the invention are particularly preferred for polyamide fibers.

Fibers which are particularly suitable according to the invention can be obtained from polyamides. The polyamides are in the patent applications WO 95/28443, WO 99/43732, EP-A-0 345 648 , WO 02/092664 and DE-A-101 23 733 described.

Polyamides are understood to mean homopolymers, copolymers, mixtures and grafts of synthetic long-chain polyamides which, as an essential constituent, have recurring amide groups in the main polymer chain. Examples of such polyamides are nylon 6 (polycaprolactam), nylon 6,6 (polyhexamethylene adipamide), nylon 4,6 (polytetramethylene adipamide), nylon 6,10 (polyhexamethylene sebacamide), nylon 7 (polyenantholactam), nylon 11 (polyundecanolactam), nylon 12 (polydodecanolactam) ). These polyamides are known to have the generic name of nylon. Polyamides also include the so-called aramids (aromatic polyamides), such as polymetaphenylene isophthalamide (NOMEX ^® fiber, US-A-3,287,324 ) or poly-paraphenylene terephthalamide (KEVLAR ^® fiber, US-A-3,671,542 ).

• – Monomere oder Oligomere eines C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₈-arylaliphatischen oder vorzugsweise aliphatischen Lactams wie Ethanolactam, Undecanolactam, Dodecanolactam oder Caprolactam,
• – Monomere oder Oligomere von C₂- bis C₂₀-, vorzugsweise C₃- bis C₁₈-Aminocarbonsäuren, wie 6-Aminocapronsäure, 11-Aminoundecansäure, sowie deren Oligomere und Salze, wie Alkalisalze, beispielsweise Lithium-, Natrium- oder Kalium-Salze,
• – C₂- bis C₂₀-, vorzugsweise C₃- bis C₁₅-Aminocarbonsäurenitrile,
• – Monomere oder Oligomere von C₂- bis C₂₀-Aminosäureamiden,
• – Ester, vorzugsweise C₁- bis C₄-Alkylester von C₂- bis C₂₀-, vorzugsweise C₃- bis C₁₈-Aminocarbonsäuren,
• – Monomere oder Oligomere eines C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₂-Alkyldiamins, mit einer C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₄-aliphatischen Dicarbonsäure, deren Mono- oder Dinitrile oder Oligomere,
• – Monomere oder Oligomere eines C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₂-Alkyldiamins, mit einer C₈- bis C₂₀-, vorzugsweise C₈- bis C₁₂-aromatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – Monomere oder Oligomere eines C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₂-Alkyldiamins, mit einer C₉- bis C₂₀-, vorzugsweise C₉- bis C₁₈-arylaliphatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – Monomere oder Oligomere eines C₆- bis C₂₀-, vorzugsweise C₆- bis C₁₀-aromatischen Diamins mit einer C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₄-aliphatischen Dicarbonsäure, deren Mono- oder Dinitrile oder Oligomere,
• – Monomere oder Oligomere eines C₆- bis C₂₀-, vorzugsweise C₆- bis C₁₀-aromatischen Diamins, mit einer C₈- bis C₂₀-, vorzugsweise C₈- bis C₁₂-aromatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – Monomere oder Oligomere eines C₆- bis C₂₀-, vorzugsweise C₆- bis C₁₀-aromatischen Diamins, mit einer C₉- bis C₂₀, vorzugsweise C₉- bis C₁₈-arylaliphatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – Monomere oder Oligomere eines C₇- bis C₂₀-, vorzugsweise C₈- bis C₁₈-arylaliphatischen Diamins mit einer C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₄-aliphatischen Dicarbonsäure, deren Mono- oder Dinitride oder Oligomere,
• – Monomere oder Oligomere eines C₇- bis C₂₀-, vorzugsweise C₈- bis C₁₈-arylaliphatischen Diamins mit einer C₆- bis C₂₀-, vorzugsweise C₆- bis C₁₀-aromatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – Monomere oder Oligomere eines C₇- bis C₂₀-, vorzugsweise C₈- bis C₁₈-arylaliphatischen Diamins mit einer C₉- bis C₂₀-, vorzugsweise C₉- bis C₁₈-arylaliphatischen Dicarbonsäure, deren Derivate oder Oligomere,
• – sowie Homopolymere, Copolymere, Mischungen und Pfropfungen solcher Ausgangsmonomere oder Ausgangsoligomere.

The preparation of these polyamides is known to the person skilled in the art and is described or mentioned, for example, in the abovementioned patent applications. The following are used as monomers:

• Monomers or oligomers of a C ₂ to C ₂₀ , preferably C ₂ to C ₁₈ arylaliphatic or preferably aliphatic lactams such as ethanolactam, undecanolactam, dodecanolactam or caprolactam,
• - Monomers or oligomers of C ₂ - to C ₂₀ -, preferably C ₃ - to C ₁₈ -aminocarboxylic acids, such as 6-aminocaproic acid, 11-aminoundecanoic acid, and their oligomers and salts, such as alkali metal salts, for example lithium, sodium or potassium salts
• C ₂ to C ₂₀ , preferably C ₃ to C ₁₅ aminocarbonsitriles,
• Monomers or oligomers of C ₂ to C ₂₀ amino acid amides,
• Esters, preferably C ₁ to C ₄ alkyl esters of C ₂ to C ₂₀ , preferably C ₃ to C ₁₈ amino carboxylic acids,
• - Monomers or oligomers of a C ₂ - to C ₂₀ -, preferably C ₂ - to C ₁₂ -alkyldiamine, with a C ₂ - to C ₂₀ -, preferably C ₂ - to C ₁₄ -aliphatic dicarboxylic acid, its mono- or dinitriles or oligomers,
• Monomers or oligomers of a C ₂ to C ₂₀ , preferably C ₂ to C ₁₂ alkyldiamine, with a C ₈ to C ₂₀ , preferably C ₈ to C ₁₂ aromatic dicarboxylic acid, its derivatives or oligomers,
• Monomers or oligomers of a C ₂ to C ₂₀ , preferably C ₂ to C ₁₂ alkyldiamine, with a C ₉ to C ₂₀ , preferably C ₉ to C ₁₈ arylaliphatic dicarboxylic acid, its derivatives or oligomers,
• - Monomers or oligomers of a C ₆ - to C ₂₀ -, preferably C ₆ - to C ₁₀ -aromatic diamine with a C ₂ - to C ₂₀ -, preferably C ₂ - to C ₁₄ -aliphatic dicarboxylic acid, its mono- or dinitriles or oligomers,
• Monomers or oligomers of a C ₆ to C ₂₀ , preferably C ₆ to C ₁₀ aromatic diamine, with a C ₈ to C ₂₀ , preferably C ₈ to C ₁₂ aromatic dicarboxylic acid, its derivatives or oligomers,
• Monomers or oligomers of a C ₆ to C ₂₀ , preferably C ₆ to C ₁₀ aromatic diamine, with a C ₉ to C ₂₀ , preferably C ₉ to C ₁₈ arylaliphatic dicarboxylic acid, its derivatives or oligomers,
• - Monomers or oligomers of a C ₇ - to C ₂₀ -, preferably C ₈ - to C ₁₈ -arylaliphatic diamine with a C ₂ - to C ₂₀ -, preferably C ₂ - to C ₁₄ -aliphatic dicarboxylic acid, their mono- or dinitrides or oligomers,
• Monomers or oligomers of a C ₇ to C ₂₀ , preferably C ₈ to C ₁₈ arylaliphatic diamine with a C ₆ to C ₂₀ , preferably C ₆ to C ₁₀ aromatic dicarboxylic acid, its derivatives or oligomers,
• Monomers or oligomers of a C ₇ to C ₂₀ , preferably C ₈ to C ₁₈ arylaliphatic diamine with a C ₉ to C ₂₀ , preferably C ₉ to C ₁₈ arylaliphatic dicarboxylic acid, their derivatives or oligomers,
• - As well as homopolymers, copolymers, mixtures and grafts of such starting monomers or starting oligomers.

In a preferred embodiment the polyamide is made from caprolactam, tetramethylene diamine, hexamethylene diamine or their mixtures and the dicarboxylic acids adipic acid, sebacic acid, dodecanedioic acid, terephthalic acid, isophthalic acid or their mixtures produced. Caprolactam is particularly preferred as lactam, as diamine hexamethylene diamine and as dicarboxylic acid adipic acid or terephthalic acid or their mixtures.

• – Monocarbonsäuren,
• – wie Alkancarbonsäuren, beispielsweise Essigsäure, Propionsäure,
• – wie Benzol- oder Naphthalinmonocarbonsäuren, beispielsweise Benzoesäure
• – Dicarbonsäure,
• – wie C₄-C₁₀-Alkandicarbonsäuren, beispielsweise Adipinsäure, Azelainsäure, Sebacinsäure, Dodecandisäure,
• – wie C₅-C₈-Cycloalkandicarbonsäuren, beispielsweise Cyclohexan-l,4-dicarbonsäure,
• – wie Benzol- oder Naphthalindicarbonsäure, beispielsweise Terephthalsäure, Isophthalsäure, Naphthalin-2,6-dicarbonsäure,
• – C₂- bis C₂₀-, vorzugsweise C₂- bis C₁₂-Alkylamine,
• – wie Cyclohexylamin, C₆- bis C₂₀-, vorzugsweise C₆- bis C₁₀-aromatische Monamine, wie Anilin, oder C₇- bis C₂₀-, vorzugsweise C₈ bis C₁₈-arylaliphatische Monamine, wie Benzylamin,
• – Diamine,
• – wie C₄-C₁₀-Alkandiamin, beispielsweise Hexamethylendiamin oder
• – wie sterisch gehinderte Piperidin-Derivate.

Chain regulators are preferably added in the production of the polyamides from which the fibers to be dyed according to the invention are produced. The following can preferably serve as chain regulators:

• - monocarboxylic acids,
• Such as alkane carboxylic acids, for example acetic acid, propionic acid,
• - Like benzene or naphthalene monocarboxylic acids, for example benzoic acid
• - dicarboxylic acid,
• Such as C ₄ -C ₁₀ alkanedicarboxylic acids, for example adipic acid, azelaic acid, sebacic acid, dodecanedioic acid,
• Such as C ₅ -C ₈ cycloalkanedicarboxylic acids, for example cyclohexane-1,4-dicarboxylic acid,
• Such as benzene or naphthalenedicarboxylic acid, for example terephthalic acid, isophthalic acid, naphthalene-2,6-dicarboxylic acid,
• C ₂ to C ₂₀ , preferably C ₂ to C ₁₂ alkylamines,
• - such as cyclohexylamine, C ₆ - to C ₂₀ -, preferably C ₆ - to C ₁₀ -aromatic monamines, such as aniline, or C ₇ - to C ₂₀ -, preferably C ₈ to C ₁₈ -arylaliphatic monamines, such as benzylamine,
• - diamines,
• - Like C ₄ -C ₁₀ alkanediamine, for example hexamethylene diamine or
• - Like sterically hindered piperidine derivatives.

The chain regulators can be unsubstituted or substituted, for example by aliphatic groups, preferably C ₁ -C ₈ -alkyl groups, such as methyl, ethyl, isopropyl, n-propyl, n-butyl, isobutyl, sec-butyl, n-pentyl, n-hexyl, n-heptyl, n-octyl, 2-ethylhexyl, OH, = O, C ₁ -C ₈ alkoxy, COOH, C ₂ -C ₆ carbalkoxy, C ₁ -C ₁₀ acyloxy, or C ₁ -C ₈ alkylamino, sulfonic acid or salts thereof, such as alkali or alkaline earth metal salts, cyano, or halogens, such as fluorine, chlorine, bromine. Examples of substituted chain regulators are sulfoisophthalic acid, its alkali metal or alkaline earth metal salts, such as lithium, sodium or potassium salts, sulfoisophthalic acid esters, for example with C ₁ -C ₁₆ -alkanols, or sulfoisophthalic acid mono- or diamides, in particular with those suitable for the formation of polyamides, monomers bearing at least one amine group, such as hexamethylenediamine or 6-aminocarboxylic acid.

You can advantageously use the chain regulator in amounts of at least 0.01 mol%, preferably at least 0.05 mol%, in particular at least 0.2 mol%, based on 1 mol of acid amide groups of the polyamide. You can advantageously use the chain regulator in quantities of at most 1.0 mol%, preferably at most 0.6 mol%, in particular at most 0.5 mol%, based on 1 mol of acid amide groups of the polyamide.

The polyamides that make up the dyes Fiber materials obtained preferably contain one the polymer chain chemically bound sterically hindered piperidine derivative. The polyamide can mixtures of such as a sterically hindered piperidine derivative contain sterically hindered piperidine derivatives.

wobei
R¹ für eine funktionelle Gruppe steht, die zur Amidbildung gegenüber der Polymerkette des Polyamids fähig ist, vorzugsweise eine Gruppe -(NH)R⁵, wobei R⁵ für Wasserstoff oder C₁-C₈-Alkyl steht, oder eine Carboxylgruppe oder ein Carboxylderivat oder eine Gruppe -(CH₂)_X(NH)R⁵, wobei X für 1 bis 6 steht und R⁵ für Wasserstoff oder C₁-C₈-Alkyl steht, oder eine Gruppe -(CH₂)_yCOOH, wobei y für 1 bis 6 steht, oder ein -(CH₂)_yCOOH Säurederivat, wobei y für 1 bis 6 steht, insbesondere für eine Gruppe – NH₂ steht,
R² für eine Alkylgruppe steht, vorzugsweise eine C₁-C₄-Alkylgruppe, wie Methyl, Ethyl, n-Propyl, Isopropyl, n-Butyl, iso-Butyl, sec.-Butyl, insbesondere eine Methylgruppe,
R³ für Wasserstoff, C₁-C₄-Alkyl oder O-R⁴ steht, wobei R⁴ für Wasserstoff oder C₁-C₇-Alkyl steht, insbesondere R³ für Wasserstoff steht.Preferred sterically hindered piperidine derivatives are those of the formula (III)

in which
R ^{1 stands} for a functional group which is capable of amide formation with respect to the polymer chain of the polyamide, preferably a group - (NH) R ⁵ , where R ^{5 stands} for hydrogen or C ₁ -C ₈ alkyl, or a carboxyl group or a carboxyl derivative or a group - (CH ₂ ) _X (NH) R ⁵ , where X is 1 to 6 and R ^{5 is} hydrogen or C ₁ -C ₈ alkyl, or a group - (CH ₂ ) _y COOH, where y represents 1 to 6, or a - (CH ₂ ) _y COOH acid derivative, where y represents 1 to 6, in particular represents a group - NH ₂ ,
R ^{2 represents} an alkyl group, preferably a C ₁ -C ₄ alkyl group, such as methyl, ethyl, n-propyl, isopropyl, n-butyl, iso-butyl, sec-butyl, in particular a methyl group,
R ^{3 is} hydrogen, C ₁ -C ₄ alkyl or OR ⁴ , where R ^{4 is} hydrogen or C ₁ -C ₇ alkyl, in particular R ^{3 is} hydrogen.

Particularly preferred as steric hindered piperidine derivative is 4-amino-2,2,6,6-tetramethylpiperidine.

This is preferably hindered Piperidine derivative in amounts of at least 0.01 mol%, especially preferably at least 0.05 mol%, in particular at least 0.1 mol%, based on 1 mole of acid amide groups of the polyamide used. Preferably you can connect of the general formula (III) in amounts of at most 0.8 mol%, particularly preferred at the most 0.6 mol%, in particular at most 0.4 mol%, based on 1 mol of acid amide groups of the polyamide.

The piperidine derivative is preferred before or during added to the polymerization.

The polymide fibers to be dyed can be used as contain a 2,6-diaminopyridine derivative. These pyridine derivatives are described for example on pages 9 to 18 of WO 02/092664.

Another subject of the present Invention are coloring agents a leveling aid according to the invention and contain at least one dye.

• (i) Bereitstellung eines erfindungsgemäßen Egalisierhilfsmittels durch Mischen von mindestens einem Aminsalz eines Arylalkylsulfonats, mindestens eines alkoxylierten Alkylamins und gegebenenfalls eines alkoxylierten Alkylalkohols,
• (ii) Zugabe von mindestens einem Farbstoff zu dem Egalisierhilfsmittel, wobei ein Färbungsmittel resultiert.

These colorants are preferably provided by a process comprising the following process steps:

• (i) Provision of a leveling aid according to the invention by mixing at least one amine salt of an arylalkyl sulfonate, at least one alkoxylated alkylamine and optionally one alkoxylated alkyl alcohol,
• (ii) adding at least one dye to the leveling aid, resulting in a colorant.

• (i) Bereitstellen einer wässrigen Lösung durch Mischen von
• (a) mindestens einem Entschäumer,
• (b) einer erfindungsgemäßen Zusammensetzung,
• (c) eines Puffersystems,
• (ii) Rühren der resultierenden wässrigen Lösung, und
• (iii) Zugabe von mindestens einem Farbstoff,

wobei ein Färbungsmittel resultiert.In a particular embodiment of the present invention, the colorant is prepared by the following process steps:

• (i) providing an aqueous solution by mixing
• (a) at least one defoamer,
• (b) a composition according to the invention,
• (c) a buffer system,
• (ii) stirring the resulting aqueous solution, and
• (iii) addition of at least one dye,

resulting in a colorant.

The provision of watery solution can preferably at temperatures of 5 to 60 ° C, particularly preferably 10 to 50 ° C, in particular 15 to 45 ° C, respectively.

Generally, by adding of the buffer system a pH of the resulting solution of 3 to 8, preferably 4 to 6, particularly preferably 5 to 6, effected. For example, an acetate buffer solution can be used as the buffer system become. More examples for Buffer systems are phosphate buffers and salts of polycarboxylic acids, dicarboxylic acids, tricarboxylic acids as well Mixtures of the aforementioned buffer systems.

As defoamers (foam preventers) can In general, all defoamers known to those skilled in the art can be used. Examples therefor are polysiloxane compounds (e.g. Respumit S) or fatty alcohol ethoxylates (e.g. Vitexol S).

The order of addition of each Components of the colorant according to the invention is arbitrary, the buffer preferably being added before the dye becomes.

Stirring the aqueous solution in process step (ii) is generally done for a period of 1 to 20 minutes, preferably 2 to 15 minutes, particularly preferably 3 to 15 minutes.

The dye is preferably pre-soaked in the aqueous solution given (process step (iii)).

As a dye in the colorant of the invention Generally all dyes are used that are suitable for dyeing Suitable for fiber materials. Examples are highly lightfast acid or metal complex dyes, such as Acid Yellow 183 and Acid Brown 355.

The amount of dye in the colorant of the invention is preferably 0.2 to 6% by weight, particularly preferably 0.3 to 4% by weight, in particular 0.4 to 3.5% by weight, based in each case on the colorant according to the invention.

The colorant of the invention is preferred at temperatures from room temperature to 100 ° C, particularly preferably 30 to 80 ° C, in particular 40 to 60 ° C, with the ones to be colored Fibers brought into contact. In a preferred embodiment of the present invention, the fiber material is first in Submitted water and then the coloring agent according to the invention is in this aqueous solution provided as described above. Alternatively, it is also possible that coloring agents according to the invention first to provide and then the one to be colored Add fiber material.

The action of the colorant according to the invention the fibers are preferably applied using a temperature gradient. For example, the coloring carried out under the following conditions:

Version 1:

• - 5th min at 40 ° C
• - With 1 ° / min to 60 ° C heat up, 20 min at 60 ° C to dye,
• - With 1 ° / min to 96 ° C heat up, 60 min at 96 ° C to dye,

Variant 2:

• - Attitude pH at 8 at 60 ° C with Eulysin WP / ammonia, at 1 ° / min to 98 ° C Heat up, with continuous pH drop to 5.3.

The amount of dye for coloring is preferably 0.2 to 1.0% by weight, particularly preferably 0.3 to 0.9% by weight, in particular 0.4 to 0.8 wt .-%, each based on the mass of the fibers.

The amount of leveling aid is preferably 1 to 10% by weight, particularly preferably 1.5 to 9% by weight, in particular 2 to 8 wt .-%, each based on the mass of the fibers.

The present invention furthermore relates to fiber materials which contain a leveling aid according to the invention or with at least one leveling aid according to the invention or with one of them coloring agents according to the invention were treated.

The invention will follow from the Examples closer explained.

embodiments

example 1

Experimental procedure:

With a fleet ratio of 1:20 and an initial temperature of 40 ° C water is presented. Then will first a defoamer and then added leveling agent and buffer system. After 5 min stirring pre-dissolved dye is added at this temperature.

Time and temperature development:

Version 1:

• - 5th min at 40 ° C
• - With 1 ° / min to 60 ° C heat up, 20 min at 60 ° C to dye,
• - With 1 ° / min to 96 ° C heat up, 60 min at 96 ° C to dye,

Variant 2:

• - Attitude pH = 8 at 60 ° C with Eulsyn WP / ammonia, at 1 ° / min to 98 ° C Heat up, with continuous pH drop to 5.3.

Then the dye liquor drained, rinsed warm and cold and dried.

Materials:

• A) Knitted polyamide yarn
• B) Polyamide yarn knitted from a polyamide with the characteristics WO 02/092664 (with 4-amino-2,2,6,6-tetramethylpiperidine)
• C) Polyamide carpet material made of a polyamide with the characteristics WO 02/092664 (with 4-amino-2,2,6,6-tetramethylpiperidine)

dyes

The percentages are% by weight and refer to the fiber material.

aids:

• 0.5-1.5 g / l Vitexol K (depending on the device)
• 2.50 wt .-% leveling agent X, based on the used fiber
• X = 1 = according to the invention
• X = 2 = tools off DE 2 343 418
• X = 3 = Uniperol AC (leveling aid without alkylarylsulfonate amine salt)

Buffer system:

• 20 ml / l acetate buffer solution. pH 5.5 * (buffer solution pH 5.5 = 70 g / l sodium acetate anhydrous and 8 ml / l acetic acid 100 %)

Rating:

Visual assessment of the levelness of dyeings without aids compared to dyeings with aids.

Example 2:

Water is introduced at a liquor ratio of 1:20 and an initial temperature of 20 ° C. and with 20 ml / l acetate buffer solution pH = 5.5 (buffer solution pH = 5.5 = 70 g / l sodium acetate + 8 ml / l acetic acid 100% ) added. A mixture of pre-dissolved dyes (0.15% Tectilon ^® Yellow 3R; 0.14% Nylamin ^® Brillant Red and Tectilon ^® Blue 4R) added. The dye liquor is heated to 95 ° C. at 3 ° C./min. Then 5% by weight of the auxiliary according to the invention was added and kept at this temperature for 2 hours. An evaluation of the color result gave a 5 (according to example 1), which illustrates the good synchronization effect of the aid according to the invention.

Comparative Example:

Water is introduced at a liquor ratio of 1:20 and an initial temperature of 20 ° C. and 20 ml / l acetate buffer solution pH = 5.5 (buffer solution pH = 5.5 = 70 g / l sodium acetate anhydrous + 8 ml / l acetic acid 100% ) added. A mixture of pre-dissolved dyes (0.15% Tectilort Yellow 3R; 0.14% Nylomin ^® Brillant Red and Tectilon ^® Blue 4R) is then added. The dye liquor is heated to 95 ° C at 3 ° C / min. Then 5% by weight of Uniperol AC was added and kept at this temperature for 2 hours. An evaluation of the dyeing result gave a 2 (according to Example 1). Even after a 6-hour residence time at this temperature, only a rating of 2-3 was achieved.

Claims (13)

Composition containing at least one amine salt an alkylarylsulfonate and at least one alkoxylated alkylamine. Composition according to claim 1, characterized in that the alkylarylsulfonate has a linear, branched or partially branched C ₁ -C ₃₆ alkyl radical and a C ₆ -C ₁₂ aryl radical. Composition according to claim 1 or 2, characterized in that the alkoxylated alkylamine is obtainable by reacting a C ₁ -C ₃₆ alkylamine with on average 2 to 100 mol of at least one C ₂ -C ₅ alkylene oxide. Composition according to one of claims 1 to 3, characterized in that the mixture additionally at least one alkoxylated Contains alkyl alcohol. Composition according to claim 4, characterized in that the alkoxylated alkyl alcohol is obtainable by reacting a C ₁ -C ₃₆ alkyl alcohol with on average 2 to 100 mol of at least one C ₂ -C ₅ alkylene oxide. Composition according to one of claims 1 to 5, characterized in that the amine salt content of an alkylarylsulfonate 20 to 70 wt .-%, the content of alkoxylated alkylamine 1 to 20 % By weight and the content of alkoxylated alkyl alcohol 0 to 20% by weight is, each based on the composition, the total weight the composition is 100% by weight. Process for the preparation of a composition according to one of the claims 1 to 6, characterized in that at least one amine salt an alkylarylsulfonate, at least one alkoxylated alkylamine and optionally at least one alkoxylated alkyl alcohol with one another mixed. Use of a composition according to claims 1 to 6 as leveling aid. Leveling agent containing a composition according to one of claims 1 to 6. Use of the leveling agent according to claim 9 for coloring of fibers. Use according to claim 10, characterized in that that the fiber is a polyamide fiber. Use according to claim 10 or 11, characterized in that that the fiber 4-amino-2,2,6,6-tetramethylpiperidine contains. Colorants, containing a leveling agent according to claim 9 and at least a dye.